関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 2-Chloro-5-(chloromethyl)pyridine | HCID 155479 | — |
| 反応物 | 2-Chloro-4-(3-trifluoromethylphenoxy)phenol | HCID 18966727 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Chloro-5-[2-chloro-4-(3-trifluoromethylphenoxy)phenoxy]methylpyridine | HCID 19798099 | — |
反応手順
To a solution 0.07 g of sodium hydride (60% oil dispersion) in 10 ml of N,N-dimethylformamide, there was added dropwise a solution of 0.50 g of 2-chloro-4-(3-trifluoromethylphenoxy)phenol in 3 ml of N,N-dimethylformamide with stirring and ice-cooling. After 30 minutes, a solution of 0.28 g of 2-chloro-5-chloromethylpyridine in 5 ml of N,N-dimethylformamide was added thereto at room temperature, followed by stirring at the same temperature for 10 hours. The reaction mixture was poured into ice-water and extracted twice with 100 ml of ethyl acetate. The extracts were combined together, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel chromatography to give 2-chloro-5-[2-chloro-4-(3-trifluoromethylphenoxy)phenoxy]methylpyridine.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05243087 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-cfef7c7616f74cf4b1c7989b7ccd6e17 |
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| 出典メモ | uspto-grants-1993_09 |
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